HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → HCID 178478198, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 3-Morpholinone | HCID 66953 | — |
| Reactant | 2-Morpholinoaniline | HCID 735756 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 178478198 | HCID 178478198 | — |
Reaction Steps
A mixture of 3-morpholinone (4 g) in dry acetonitrile (40 ml), 4-(2-aminophenyl)morpholine (3.6 g) in dry acetonitrile (20 ml) and phosphorous oxychloride (3.6 ml) was heated for 40 hours at 65°-70° C. to give oil which was purified by column chromatography on neutral alumina (72 g) using (a) hexane, (b) dichloromethane:hexane (1:1) and (c) dichloromethane as eluant. The resulting oil was treated with a saturated solution of hydrogen chloride in methanol (25 ml) to give a pale yellow solid which was recrystallised from a 1:1 mixture of methanol and ether to give 4-[2-(3-morpholinylideneamino)phenyl]-morpholine hydrochloride (m.p. 262°-263° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05373008 |
| Source dataset | uspto-grants-1994_12 |
| ORD ID | ord-32be69fe9dcf42aab300f5aea813480b |
| Source note | uspto-grants-1994_12 |